HRID247110

反应详情

EQUATION

反应方程式

HRID 247110 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 15.0 g of 5-acetonyl-3-chloromethyl-1,2,4-oxadiazole in 50 ml of THF were added dropwise 17.4 g of triethylamine and subsequently 11.0 g of piperidine. The mixture was stirred at room temperature for 24 hours and then heated under reflux for 6 hours. After cooling, the precipitated material was removed by filtration and the filtrate was evaporated in vacuo. The residue was chromatographed on silica gel using chloroform-methanol (20:1, v/v) as eluent to give 10.9 g of 5-acetonyl-3-piperidinomethyl-1,2,4-oxadiazole as a colorless solid, m.p. 66°-67° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 6 hours
  3. temperatureAfter cooling
  4. customthe precipitated material was removed by filtration
  5. customthe filtrate was evaporated in vacuo
  6. customThe residue was chromatographed on silica gel